EP0595084A1 - Apparatus for carrying out chemical reactions - Google Patents

Apparatus for carrying out chemical reactions Download PDF

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Publication number
EP0595084A1
EP0595084A1 EP93116162A EP93116162A EP0595084A1 EP 0595084 A1 EP0595084 A1 EP 0595084A1 EP 93116162 A EP93116162 A EP 93116162A EP 93116162 A EP93116162 A EP 93116162A EP 0595084 A1 EP0595084 A1 EP 0595084A1
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EP
European Patent Office
Prior art keywords
enclosure
reactor
neck
passage
microwave
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP93116162A
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German (de)
French (fr)
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EP0595084B1 (en
Inventor
Sylvain Jean-Marie Rault
Jean-Claude Derobert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Universite de Caen Normandie
Moulinex SA
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Universite de Caen Normandie
Moulinex SA
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/80—Apparatus for specific applications
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/19—Details relating to the geometry of the reactor
    • B01J2219/194—Details relating to the geometry of the reactor round
    • B01J2219/1941—Details relating to the geometry of the reactor round circular or disk-shaped
    • B01J2219/1942—Details relating to the geometry of the reactor round circular or disk-shaped spherical
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S422/00—Chemical apparatus and process disinfecting, deodorizing, preserving, or sterilizing
    • Y10S422/906—Plasma or ion generation means

Definitions

  • the invention relates to a device for conducting chemical operations comprising a working enclosure delimited by a vault, a silk, side walls and a door, a microwave energy generator for said enclosure and a reactor having at least one neck and resting in said enclosure on a support.
  • the object of the present invention is to provide a device which can carry out all the current operations of chemistry in a manner similar to those which are carried out in a conventional laboratory.
  • the enclosure is pierced with at least one passage which makes it possible to relate the neck of the reactor with a connecting pipe secured to an external device for conducting a chemical reaction.
  • the invention it is possible to conduct the chemical reaction in the reactor from outside the enclosure and in particular to carry out either constant volume operations in which the external device comprises a steam condenser and a liquid injector, or distillation operations in which the external device comprises a distillation column and a liquid injector.
  • the reactor can be replaced by a coil, the ends of which are respectively connected to two through holes made in the enclosure, thus making it possible to carry out continuous syntheses.
  • the device represented in FIGS. 1 and 2 comprises a working enclosure 1 delimited by an arch 2, a hearth 3, side walls 4, 5 and a door (not shown), a microwave energy generator 6 for said enclosure, and an open type reactor 7 having at least one neck 8 and resting in said enclosure 1 by means of a support 9.
  • This enclosure 1 can be conventionally equipped with a rotary wave stirrer 10, as well as an infrared temperature detector 11 intended to ensure automatic control of the generator 6.
  • This generator 6 can operate, either at continuous power, or at variable or sequentially variable power, this as a function of the chemical reactions to be developed.
  • the reactor can have all the forms known per se in the field of chemistry and in particular present a spherical shape as illustrated.
  • the enclosure 1 is pierced with at least one passage 12 which makes it possible to relate the neck 8 of the reactor 7 with a connecting pipe 13 secured to an external device 14 for conducting the chemical reaction.
  • the vault 2 of the enclosure 1 is pierced with three passages, the passage 12 arranged vertically and two other lateral passages 15 and 16 intended respectively to allow connections with the necks of a standard type balloon, that is to say the neck 8 directed vertically and the necks 17 and 18 oriented properly.
  • These passages 12, 15 and 16 each include a device for suppressing microwave leaks outside the enclosure. Said passages are formed by tubes 12 ′, 15 ′, 16 ′ which open into orifices 19, 20, 21 formed for example in the vault 2 of the enclosure.
  • each tube 12 ′, 15 ′, 16 ′ is mounted articulated for example by means of a ball joint, on the enclosure so as to allow articulation with the necks of different types of balloons .
  • These tubes therefore constitute waveguides at the cut-off and make it possible to attenuate the electromagnetic waves to make these outputs compatible with the safety standards in force.
  • This attenuation of waves in a cylindrical tube is known per se and depends on two factors a / ⁇ o and z / a where a is the radius of the tube, z is the axial length, and ⁇ o represents the wavelength to be attenuated.
  • the method of calculation has for example been described in the book by Mc GRAW - HILL BOOK Company 1957 entitled “Microwave Measurements” by EL GINZTON.
  • the device is used to perform reactions at constant volume.
  • the external device 14 for this purpose comprises a steam condenser 22, the duct 13 of which passes through the tube 12 'and penetrates in a substantially sealed manner into the neck 8 of the reactor 7, and which is cooled by a circulation of water 23 condensing the vapors solvent.
  • the liquid thus formed returns to the reactor 7 which thus retains practically a constant volume of liquid.
  • the tubes 15 'and 16' allow respectively the passage of a thermometer or a probe 24 to penetrate in a sealed manner in the neck 17, and the passage of a conduit 25 in the neck 18 to introduce during the reaction of the solids , gas or liquid, said conduit 25 being equipped with an open-close valve 40.
  • the device is used to carry out reactions with distillation and for this purpose comprises a distillation column 26 the conduit 13 of which crosses the tube 12 'and penetrates in a sealed manner in the neck 8 of the reactor 7, and which is cooled by a circulation of water 27, the distilled liquid flowing through the orifice 28.
  • the tubes 15 ′ and 16 ′ respectively allow the thermometer or the probe 24 to pass through the neck 17, and the passage of a liquid inlet conduit 25. Thanks to this embodiment, it is also possible to envisage continuously treating a large quantity of liquid comprising, for example, a solvent and reagents, the distillation making it possible to recover the solvent while the products accompanying it accumulate at the bottom of the reactor. This achievement allows the rectification and recovery of solvents.
  • the invention provides that the hearth wall 3 has an adequate elevation 30 intended to place the reactor in the working position in the central region of the enclosure 1. Thanks to this elevation , it is possible to use reactors of the open type and of a slightly different volume, while keeping a defined type of support; that is to say a support having properties in the microwave such as: low charge, permeability, stability, dielectric material ...
  • a support 9 comprises a tank 31 preferably made of glass transparent to microwaves containing a pulverulent material 32 such as, for example, "Fontainebleau" sand.
  • said support 9 may have a certain load so as to be able to process small volumes.
  • the invention provides for fitting the enclosure 1 with a magnetic stirrer comprising a rotary motor member 33 arranged in the elevation 30 and a magnet 34 arranged in the reactor 7.
  • a magnetic stirrer comprising a rotary motor member 33 arranged in the elevation 30 and a magnet 34 arranged in the reactor 7.
  • the bottom wall 3 is preferably made of a non-magnetic material.
  • the sole is made of stainless steel.
  • the device according to the invention makes it possible to use open reactors of large volume to carry out organic synthesis reactions which, under normal laboratory conditions, could not be obtained or would be obtained with very low yields, less than 5 %.
  • a reaction of the type Such a device because of its possibility of conducting the reaction through the passages of the enclosure also allows the preparation of new compounds mainly in heterocyclic chemistry.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Toxicology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
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  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

Reaction apparatus comprising a work enclosure (1) bounded by a vault (2), a bottom (3), side walls (4, 5) and a door, a microwave energy generator (6) for the said enclosure, and a reactor (7) which has at least one neck (8) and which rests on a support (9) in the said enclosure. According to the invention the enclosure (1) is pierced with at least one passage (12) which allows the neck (8) of the reactor (7) to be placed in relation with a connecting conduit (13) integrally attached to an external device for carrying out a chemical reaction. <IMAGE>

Description

L'invention se rapporte à un dispositif de conduite d'opérations chimiques comportant une enceinte de travail délimitée par une voûte, une soie, des parois latérales et une porte, un générateur d'énergie à micro-ondes pour ladite enceinte et un réacteur ayant au moins un col et reposant dans ladite enceinte sur un support.The invention relates to a device for conducting chemical operations comprising a working enclosure delimited by a vault, a silk, side walls and a door, a microwave energy generator for said enclosure and a reactor having at least one neck and resting in said enclosure on a support.

Jusqu'à présent, un tel dispositif ne permettait de réaliser que des réactions à très faible volume et sans possibilité de conduire lesdites réactions. En fait, un tel dispositif ne permet que d'effectuer des essais, généralement en réacteur hermétiquement fermé et protégé, et de mettre en valeur l'accélération de synthèses chimiques sous l'effet du chauffage à micro-ondes.Until now, such a device has only made it possible to carry out reactions at very low volume and without the possibility of carrying out said reactions. In fact, such a device only makes it possible to carry out tests, generally in a hermetically sealed and protected reactor, and to enhance the acceleration of chemical syntheses under the effect of microwave heating.

La présente invention a pour but de réaliser un dispositif qui puisse conduire toutes les opérations courantes de la chimie de manière analogue à celles qui sont conduites dans un laboratoire classique.The object of the present invention is to provide a device which can carry out all the current operations of chemistry in a manner similar to those which are carried out in a conventional laboratory.

Selon l'invention, l'enceinte est percée d'au moins un passage qui permet de mettre en relation le col du réacteur avec un conduit de liaison solidaire d'un dispositif externe de conduite d'une réaction chimique.According to the invention, the enclosure is pierced with at least one passage which makes it possible to relate the neck of the reactor with a connecting pipe secured to an external device for conducting a chemical reaction.

Grâce à l'invention, on peut conduire de l'extérieur de l'enceinte la réaction chimique dans le réacteur et réaliser notamment soit des opérations à volume constant dans lesquelles le dispositif externe comprend un condenseur de vapeur et un injecteur de liquide, soit des opérations avec distillation dans lesquelles le dispositif externe comprend une colonne à distiller et un injecteur de liquide.Thanks to the invention, it is possible to conduct the chemical reaction in the reactor from outside the enclosure and in particular to carry out either constant volume operations in which the external device comprises a steam condenser and a liquid injector, or distillation operations in which the external device comprises a distillation column and a liquid injector.

Selon une variante de réalisation, le réacteur peut être remplacé par un serpentin dont les extrémités sont reliées respectivement à deux trous de passage pratiqués dans l'enceinte permettant ainsi d'effectuer des synthèses en continu.According to an alternative embodiment, the reactor can be replaced by a coil, the ends of which are respectively connected to two through holes made in the enclosure, thus making it possible to carry out continuous syntheses.

Les caractéristiques et avantages de l'invention ressortiront d'ailleurs de la description qui va suivre, à titre d'exemple, en référence aux dessins annexés dans lesquels :

  • La figure 1 est une coupe verticale schématique d'un dispositif selon l'invention utilisé pour accomplir des réactions à volume constant ; la figure 2 est une vue analogue du dispositif illustré à la figure 1, mais utilisé pour accomplir des réactions avec distillation.
The characteristics and advantages of the invention will become apparent from the description which follows, by way of example, with reference to the appended drawings in which:
  • Figure 1 is a schematic vertical section of a device according to the invention used to perform reactions at constant volume; Figure 2 is a similar view of the device illustrated in Figure 1, but used to perform reactions with distillation.

Le dispositif représenté aux figures 1 et 2 comporte une enceinte de travail 1 délimitée par une voûte 2, une sole 3, des parois latérales 4, 5 et une porte (non représentée), un générateur 6 d'énergie à micro-ondes pour ladite enceinte, et un réacteur 7 de type ouvert ayant au moins un col 8 et reposant dans ladite enceinte 1 au moyen d'un support 9. Cette enceinte 1 peut être équipée de façon classique d'un brasseur d'ondes rotatif 10, ainsi que d'un détecteur de température à infrarouge 11 destiné à assurer un pilotage automatique du générateur 6. Ce générateur 6 peut fonctionner, soit à puissance continue, soit à puissance variable ou variable séquentiellement, ceci en fonction des réactions chimiques à développer. Le réacteur peut présenter toutes les formes connues en soi dans le domaine de la chimie et notamment présenter une forme sphérique telle qu'illustrée.The device represented in FIGS. 1 and 2 comprises a working enclosure 1 delimited by an arch 2, a hearth 3, side walls 4, 5 and a door (not shown), a microwave energy generator 6 for said enclosure, and an open type reactor 7 having at least one neck 8 and resting in said enclosure 1 by means of a support 9. This enclosure 1 can be conventionally equipped with a rotary wave stirrer 10, as well as an infrared temperature detector 11 intended to ensure automatic control of the generator 6. This generator 6 can operate, either at continuous power, or at variable or sequentially variable power, this as a function of the chemical reactions to be developed. The reactor can have all the forms known per se in the field of chemistry and in particular present a spherical shape as illustrated.

Selon l'invention, l'enceinte 1 est percée d'au moins un passage 12 qui permet de mettre en relation le col 8 du réacteur 7 avec un conduit de liaison 13 solidaire d'un dispositif externe 14 de conduite de la réaction chimique.According to the invention, the enclosure 1 is pierced with at least one passage 12 which makes it possible to relate the neck 8 of the reactor 7 with a connecting pipe 13 secured to an external device 14 for conducting the chemical reaction.

Comme on le voit sur les figures 1 et 2, la voûte 2 de l'enceinte 1 est percée de trois passages, le passage 12 agencé verticalement et deux autres passages latéraux 15 et 16 destinés respectivement à permettre des liaisons avec les cols d'un ballon de type standard, c'est-à-dire le col 8 dirigé verticalement et les cols 17 et 18 orientés convenablement. Ces passages 12, 15 et 16 comportent chacun un dispositif de suppression des fuites micro-ondes hors de l'enceinte. Lesdits passages sont formés par des tubes 12', 15', 16' qui débouchent dans des orifices 19, 20, 21 pratiqués par exemple dans la voûte 2 de l'enceinte.As seen in Figures 1 and 2, the vault 2 of the enclosure 1 is pierced with three passages, the passage 12 arranged vertically and two other lateral passages 15 and 16 intended respectively to allow connections with the necks of a standard type balloon, that is to say the neck 8 directed vertically and the necks 17 and 18 oriented properly. These passages 12, 15 and 16 each include a device for suppressing microwave leaks outside the enclosure. Said passages are formed by tubes 12 ′, 15 ′, 16 ′ which open into orifices 19, 20, 21 formed for example in the vault 2 of the enclosure.

Selon une variante de réalisation non représentée, chaque tube 12', 15', 16' est monté articulé par exemple au moyen d'une liaison à rotule, sur l'enceinte de manière à permettre une articulation avec les cols de différents types de ballons. Ces tubes constituent donc des guides d'ondes à la coupure et permettent d'atténuer les ondes électromagnétiques pour rendre ces sorties compatibles avec les normes de sécurité en vigueur. Cette atténuation des ondes dans un tube cylindrique est connue en soi et dépend de deux facteurs a/λo et z/a où a est le rayon du tube, z est la longueur axiale, et λo représente la longueur d'onde à atténuer. Le choix du rayon du guide est tel que la longueur de l'onde à atténuer λo soit plus grande que la longueur d'onde de coupure du mode TEM. Par exemple pour une onde λo = 12,2 cm, on choisira a = 2 cm et z = 20 cm. Le mode de calcul a par exemple été décrit dans le livre de Mc GRAW - HILL BOOK Company 1957 intitulé "Microwave Measurements" de E.L. GINZTON.According to a variant embodiment not shown, each tube 12 ′, 15 ′, 16 ′ is mounted articulated for example by means of a ball joint, on the enclosure so as to allow articulation with the necks of different types of balloons . These tubes therefore constitute waveguides at the cut-off and make it possible to attenuate the electromagnetic waves to make these outputs compatible with the safety standards in force. This attenuation of waves in a cylindrical tube is known per se and depends on two factors a / λo and z / a where a is the radius of the tube, z is the axial length, and λo represents the wavelength to be attenuated. The choice of the radius of the guide is such that the length of the wave to be attenuated λo is greater than the cut-off wavelength in TEM mode. For example, for a wave λo = 12.2 cm, we will choose a = 2 cm and z = 20 cm. The method of calculation has for example been described in the book by Mc GRAW - HILL BOOK Company 1957 entitled "Microwave Measurements" by EL GINZTON.

Grâce à ces tubes accordés, on comprend que l'utilisation de réacteurs ouverts ne pose aucun problème à l'utilisateur et permet donc de conduire toutes les opérations courantes de la chimie et plus particulièrement celles de la chimie de synthèse organique.Thanks to these tuned tubes, it is understood that the use of open reactors poses no problem to the user and therefore makes it possible to conduct all the current operations of chemistry and more particularly those of organic synthetic chemistry.

Selon une première réalisation illustrée à la figure 1, le dispositif est utilisé pour accomplir des réactions à volume constant. Le dispositif externe 14 comporte à cet effet un condenseur de vapeur 22 dont le conduit 13 traverse le tube 12' et pénètre de façon sensiblement étanche dans le col 8 du réacteur 7, et qui est refroidi par une circulation d'eau 23 condensant les vapeurs de solvant. Le liquide ainsi formé retourne dans le réacteur 7 qui conserve ainsi pratiquement un volume de liquide constant. Les tubes 15' et 16' permettent respectivement le passage d'un thermomètre ou d'une sonde 24 pour pénétrer de façon étanche dans le col 17, et le passage d'un conduit 25 dans le col 18 pour introduire pendant la réaction des solides, gaz ou liquides, ledit conduit 25 étant équipé d'une vanne d'ouverture-fermeture 40.According to a first embodiment illustrated in Figure 1, the device is used to perform reactions at constant volume. The external device 14 for this purpose comprises a steam condenser 22, the duct 13 of which passes through the tube 12 'and penetrates in a substantially sealed manner into the neck 8 of the reactor 7, and which is cooled by a circulation of water 23 condensing the vapors solvent. The liquid thus formed returns to the reactor 7 which thus retains practically a constant volume of liquid. The tubes 15 'and 16' allow respectively the passage of a thermometer or a probe 24 to penetrate in a sealed manner in the neck 17, and the passage of a conduit 25 in the neck 18 to introduce during the reaction of the solids , gas or liquid, said conduit 25 being equipped with an open-close valve 40.

Selon une seconde réalisation illustrée à la figure 2, le dispositif est utilisé pour réaliser des réactions avec distillation et comporte à cet effet une colonne à distiller 26 dont le conduit 13 traverse le tube 12' et pénètre de façon étanche dans le col 8 du réacteur 7, et qui est refroidie par une circulation d'eau 27, le liquide distillé s'écoulant par l'orifice 28. Les tubes 15' et 16' permettent respectivement le passage par le col 17 du thermomètre ou de la sonde 24, et le passage d'un conduit 25 d'arrivée de liquide.
Grâce à cette réalisation on peut également envisager de traiter en continu une grande quantité de liquide comprenant, par exemple, un solvant et des réactifs, la distillation permettant de récupérer le solvant tandis que les produits l'accompagnant s'accumulent au fond du réacteur. Cette réalisation permet la rectification et la récupération de solvants.According to a second embodiment illustrated in FIG. 2, the device is used to carry out reactions with distillation and for this purpose comprises a distillation column 26 the conduit 13 of which crosses the tube 12 'and penetrates in a sealed manner in the neck 8 of the reactor 7, and which is cooled by a circulation of water 27, the distilled liquid flowing through the orifice 28. The tubes 15 ′ and 16 ′ respectively allow the thermometer or the probe 24 to pass through the neck 17, and the passage of a liquid inlet conduit 25.
Thanks to this embodiment, it is also possible to envisage continuously treating a large quantity of liquid comprising, for example, a solvent and reagents, the distillation making it possible to recover the solvent while the products accompanying it accumulate at the bottom of the reactor. This achievement allows the rectification and recovery of solvents.

Afin d'améliorer les réactions au sein du réacteur 7, l'invention prévoit que la paroi de sole 3 présente une surélévation adéquate 30 destinée à placer le réacteur en position de travail dans la région centrale de l'enceinte 1. Grâce à cette surélévation, on peut utiliser des réacteurs de type ouvert et de volume un peu différent, tout en gardant un support de type défini ; c'est-à-dire un support présentant des propriétés aux micro-ondes telles que : faible charge, perméabilité, stabilité, matériau diélectrique... Un tel support 9 comporte un bac 31 de préférence en verre transparent aux micro-ondes contenant un matériau pulvérulent 32 tel que, par exemple, du sable "de Fontainebleau".In order to improve the reactions within the reactor 7, the invention provides that the hearth wall 3 has an adequate elevation 30 intended to place the reactor in the working position in the central region of the enclosure 1. Thanks to this elevation , it is possible to use reactors of the open type and of a slightly different volume, while keeping a defined type of support; that is to say a support having properties in the microwave such as: low charge, permeability, stability, dielectric material ... Such a support 9 comprises a tank 31 preferably made of glass transparent to microwaves containing a pulverulent material 32 such as, for example, "Fontainebleau" sand.

Dans un autre exemple de réalisation non représenté, ledit support 9 peut présenter une certaine charge de manière à pouvoir traiter des petits volumes.In another exemplary embodiment not shown, said support 9 may have a certain load so as to be able to process small volumes.

Dans un mode de réalisation préféré et afin d'obtenir une bonne homogénéisation du contenu du réacteur 7, l'invention prévoit d'équiper l'enceinte 1 d'un agitateur magnétique comportant un organe moteur rotatif 33 agencé dans la surélévation 30 et un aimant 34 agencé dans le réacteur 7. A cet effet, la paroi de sole 3 est réalisée de préférence en un matériau non magnétique. De préférence pour des raisons de tenue en température, de rigidité et de propreté, la sole est réalisée en acier inoxydable.In a preferred embodiment and in order to obtain good homogenization of the contents of the reactor 7, the invention provides for fitting the enclosure 1 with a magnetic stirrer comprising a rotary motor member 33 arranged in the elevation 30 and a magnet 34 arranged in the reactor 7. For this purpose, the bottom wall 3 is preferably made of a non-magnetic material. Preferably for reasons of temperature resistance, rigidity and cleanliness, the sole is made of stainless steel.

Ainsi le dispositif selon l'invention permet d'utiliser des réacteurs ouverts de volume important pour réaliser des réactions de synthèse organique qui, dans des conditions normales de laboratoire, ne pourraient pas être obtenues ou seraient obtenues avec de très faibles rendements, inférieurs à 5 %. Par exemple, on peut réaliser une réaction du type :

Figure imgb0001

Un tel dispositif du fait de sa possibilité de conduite de la réaction au travers des passages de l'enceinte permet aussi la préparation de composés nouveaux principalement en chimie hétérocyclique.Thus the device according to the invention makes it possible to use open reactors of large volume to carry out organic synthesis reactions which, under normal laboratory conditions, could not be obtained or would be obtained with very low yields, less than 5 %. For example, one can carry out a reaction of the type:
Figure imgb0001
Such a device because of its possibility of conducting the reaction through the passages of the enclosure also allows the preparation of new compounds mainly in heterocyclic chemistry.

En outre, des réactions du type :

Figure imgb0002

ou du type
Figure imgb0003
peuvent être réalisées avec des rendements quasiquantitatifs [ρ = 50 à 85% sur des quantités de l'ordre de 100 grammes] sous une application micro-ondes pendant 5 mn.In addition, reactions of the type:
Figure imgb0002
or of the type
Figure imgb0003
can be carried out with almost quantitative yields [ρ = 50 to 85% on quantities of the order of 100 grams] under a microwave application for 5 min.

Grâce au dispositif selon l'invention, on comprendra que l'on peut envisager des applications industrielles.Thanks to the device according to the invention, it will be understood that industrial applications can be envisaged.

Claims (10)

Dispositif de conduite d'opérations chimiques comportant une enceinte de travail (1) délimitée par une voûte (2), une sole (3), des parois latérales (4, 5) et une porte, un générateur (6) d'énergie à micro-ondes pour ladite enceinte, et un réacteur (7) ayant au moins un col (8) et reposant dans ladite enceinte sur un support (9),
caractérisé en ce que l'enceinte (1) est percée d'au moins un passage (12) que permet de mettre en relation le col (8) du réacteur (7) avec un conduit de liaison (13) solidaire d'un dispositif externe de conduite d'une réaction chimique.Device for conducting chemical operations comprising a working enclosure (1) delimited by a vault (2), a hearth (3), side walls (4, 5) and a door, a generator (6) of energy to microwave for said enclosure, and a reactor (7) having at least one neck (8) and resting in said enclosure on a support (9),
characterized in that the enclosure (1) is pierced with at least one passage (12) which makes it possible to relate the neck (8) of the reactor (7) to a connecting duct (13) secured to a device external conduct of a chemical reaction. Dispositif selon la revendication 1,
caractérisé en ce que l'enceinte est percée de deux autres passages (15 et 16) destinés respectivement à permettre des liaisons avec deux autres cols (17 et 18) du réacteur 7.Device according to claim 1,
characterized in that the enclosure is pierced with two other passages (15 and 16) intended respectively to allow connections with two other necks (17 and 18) of the reactor 7. Dispositif selon la revendication 1 ou 2,
caractérisé en ce que chaque passage (12, 15, 16) comporte un dispositif de suppression des fuites micro-ondes hors de l'enceinte.Device according to claim 1 or 2,
characterized in that each passage (12, 15, 16) comprises a device for suppressing microwave leaks outside the enclosure. Dispositif selon la revendication 3,
caractérisé en ce que chaque passage (12, 15, 16) comporte un tube (12', 15', 16') de dimension appropriée qui constitue à la fois un guide de liaison et le dispositif de suppression des fuites micro-ondes.Device according to claim 3,
characterized in that each passage (12, 15, 16) comprises a tube (12 ', 15', 16 ') of suitable size which constitutes both a connection guide and the device for suppressing microwave leaks. Dispositif selon la revendication 4,
caractérisé en ce que les tubes (12', 15', 16') sont montés articulés sur l'enceinte (1) de manière à permettre les liaisons avec différents cols de ballons.Device according to claim 4,
characterized in that the tubes (12 ', 15', 16 ') are mounted articulated on the enclosure (1) so as to allow connections with different necks of balloons. Dispositif selon l'une quelconque des revendications précédentes,
caractérisé en ce que le support (9) comporte un bac (31) transparent au micro-ondes et contenant un matériau pulvérulent (32).Device according to any one of the preceding claims,
characterized in that the support (9) comprises a container (31) transparent to the microwave and containing a material powdery (32). Dispositif selon la revendication 6,
caractérisé en ce que le matériau pulvérulent (32) est du sable.Device according to claim 6,
characterized in that the pulverulent material (32) is sand. Dispositif selon l'une quelconque des revendications précédentes,
caractérisé en ce que la sole (3) de l'enceinte (1) présente une surélévation (30) de hauteur telle que le réacteur (7) soit placé dans l'espace central de ladite enceinte (1).Device according to any one of the preceding claims,
characterized in that the floor (3) of the enclosure (1) has a height elevation (30) such that the reactor (7) is placed in the central space of said enclosure (1). Dispositif selon l'une quelconque des revendications précédentes,
caractérisé en ce que l'enceinte (1) est équipée d'un agitateur magnétique (33, 34) pour le réacteur (7), et la sole (3) est constituée en un matériau non magnétique.Device according to any one of the preceding claims,
characterized in that the enclosure (1) is equipped with a magnetic stirrer (33, 34) for the reactor (7), and the hearth (3) is made of a non-magnetic material. Dispositif selon les revendications 8 et 9,
caractérisé en ce que l'agitateur magnétique (33, 34) comprend un organe moteur (33) agencé dans la surélévation (30).Device according to claims 8 and 9,
characterized in that the magnetic stirrer (33, 34) comprises a motor member (33) arranged in the elevation (30).
EP93116162A 1992-10-30 1993-10-06 Microwave apparatus for carrying out chemical reactions Expired - Lifetime EP0595084B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9213046A FR2697448B1 (en) 1992-10-30 1992-10-30 Device for conducting chemical operations.
FR9213046 1992-10-30

Publications (2)

Publication Number Publication Date
EP0595084A1 true EP0595084A1 (en) 1994-05-04
EP0595084B1 EP0595084B1 (en) 1998-02-18

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ID=9435047

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93116162A Expired - Lifetime EP0595084B1 (en) 1992-10-30 1993-10-06 Microwave apparatus for carrying out chemical reactions

Country Status (4)

Country Link
US (1) US5659874A (en)
EP (1) EP0595084B1 (en)
DE (1) DE69317032T2 (en)
FR (1) FR2697448B1 (en)

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WO1997013137A2 (en) * 1995-10-03 1997-04-10 Cem Corporation Microwave assisted chemical processes
WO1997026064A1 (en) * 1996-01-17 1997-07-24 Tauw Milieu B.V. Method for processing a sample
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EP0872464A1 (en) * 1997-04-17 1998-10-21 Bend Research, Inc. Preparation of bioactive compounds by plasma synthesis
EP0879637A2 (en) * 1997-05-22 1998-11-25 PRO-C-EPT, naamloze vennootschap Method and device for treating a small quantity of a product
FR2873120A1 (en) * 2004-07-19 2006-01-20 Univ Littoral Cote D Opale Synthesis of cyclodextrin amino derivative, useful to prepare beta cyclodextrin derivatives, comprises subjecting tosyl derivative and sodium azide in water, applying microwaves, subjecting e.g. solvent and exposing to microwaves
CN102128740A (en) * 2010-11-22 2011-07-20 中国科学院东北地理与农业生态研究所 High-efficiency negative-pressure magnetic stirring concentration device
CN106669565A (en) * 2016-11-30 2017-05-17 重庆双丰化工有限公司 Anti-wall-adhering reaction kettle
CN106669566A (en) * 2017-02-07 2017-05-17 重庆双丰化工有限公司 Chemical reaction device for stirring
AT522473B1 (en) * 2019-06-13 2020-11-15 Anton Paar Gmbh Microwave apparatus with safe passage of electrically conductive fluids

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CN110292899B (en) * 2019-04-19 2021-06-08 东南大学 High-temperature microwave reaction kettle combined device and reaction method

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US5932075A (en) * 1993-10-28 1999-08-03 Commonwealth Scientific And Industrial Research Organisation Batch microwave reactor
WO1995011750A1 (en) * 1993-10-28 1995-05-04 Commonwealth Scientific And Industrial Research Organisation Batch microwave reactor
WO1997013137A2 (en) * 1995-10-03 1997-04-10 Cem Corporation Microwave assisted chemical processes
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US5840583A (en) * 1995-10-03 1998-11-24 Cem Corporation Microwave assisted chemical processes
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US6114680A (en) * 1996-01-17 2000-09-05 Perkin Elmer Llc Method for processing a sample
FR2760879A1 (en) * 1997-03-13 1998-09-18 Jeulin Sa Bio-reactor e.g. for teaching purposes
EP0872464A1 (en) * 1997-04-17 1998-10-21 Bend Research, Inc. Preparation of bioactive compounds by plasma synthesis
EP0879637A2 (en) * 1997-05-22 1998-11-25 PRO-C-EPT, naamloze vennootschap Method and device for treating a small quantity of a product
EP0879637A3 (en) * 1997-05-22 1999-12-15 PRO-C-EPT, naamloze vennootschap Method and device for treating a small quantity of a product
FR2873120A1 (en) * 2004-07-19 2006-01-20 Univ Littoral Cote D Opale Synthesis of cyclodextrin amino derivative, useful to prepare beta cyclodextrin derivatives, comprises subjecting tosyl derivative and sodium azide in water, applying microwaves, subjecting e.g. solvent and exposing to microwaves
CN102128740A (en) * 2010-11-22 2011-07-20 中国科学院东北地理与农业生态研究所 High-efficiency negative-pressure magnetic stirring concentration device
CN102128740B (en) * 2010-11-22 2015-12-16 中国科学院东北地理与农业生态研究所 A kind of high-efficiency negative-pressure magnetic stirring concentration device
CN106669565A (en) * 2016-11-30 2017-05-17 重庆双丰化工有限公司 Anti-wall-adhering reaction kettle
CN106669566A (en) * 2017-02-07 2017-05-17 重庆双丰化工有限公司 Chemical reaction device for stirring
AT522473B1 (en) * 2019-06-13 2020-11-15 Anton Paar Gmbh Microwave apparatus with safe passage of electrically conductive fluids
AT522473A4 (en) * 2019-06-13 2020-11-15 Anton Paar Gmbh Microwave apparatus with safe passage of electrically conductive fluids

Also Published As

Publication number Publication date
EP0595084B1 (en) 1998-02-18
FR2697448B1 (en) 1995-06-16
FR2697448A1 (en) 1994-05-06
US5659874A (en) 1997-08-19
DE69317032D1 (en) 1998-03-26
DE69317032T2 (en) 1998-06-25

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